WO2017054782A1 - 一种透射电镜双倾原位纳米压痕平台 - Google Patents

一种透射电镜双倾原位纳米压痕平台 Download PDF

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WO2017054782A1
WO2017054782A1 PCT/CN2016/105381 CN2016105381W WO2017054782A1 WO 2017054782 A1 WO2017054782 A1 WO 2017054782A1 CN 2016105381 W CN2016105381 W CN 2016105381W WO 2017054782 A1 WO2017054782 A1 WO 2017054782A1
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situ
platform
nanoindentation
tem
sample
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French (fr)
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韩晓东
李志鹏
毛圣成
王晓冬
庄春强
张剑飞
邓青松
翟亚迪
张韬楠
张泽
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Beijing University of Technology
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
    • G01N23/04—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/02—Details
    • H01J37/20—Means for supporting or positioning the object or the material; Means for adjusting diaphragms or lenses associated with the support
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/30—Accessories, mechanical or electrical features
    • G01N2223/307—Accessories, mechanical or electrical features cuvettes-sample holders
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/30—Accessories, mechanical or electrical features
    • G01N2223/32—Accessories, mechanical or electrical features adjustments of elements during operation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/40—Imaging
    • G01N2223/418—Imaging electron microscope
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
    • H01J2237/2007—Holding mechanisms
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
    • H01J2237/206—Modifying objects while observing
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
    • H01J2237/206—Modifying objects while observing
    • H01J2237/2062—Mechanical constraints
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/26—Electron or ion microscopes
    • H01J2237/262—Non-scanning techniques

Definitions

  • the invention relates to a platform for performing in-situ nanoindentation, compression and bending of materials under biaxial tilting conditions in a transmission electron microscope.
  • the sub-angstrom, nanometer and atomic scale observations of the microstructure evolution during the deformation process of the sample were realized by transmission electron microscopy. It belongs to the field of mechanical properties of nanomaterials in transmission electron microscopy - in situ characterization of microstructures.
  • Transmission electron microscopy can study the microstructure of materials at the sub-angstrom, nanometer, and atomic scales. The latest spherical aberration transmission electron microscopy has been able to study the microstructure of materials with spatial resolution less than 0.1 nm.
  • Various in-situ characterization techniques combined with TEM have been developed to study the microstructure and various properties of materials, including material mechanics, thermal, electrical, optical, and various coupling properties, greatly enriching the materials. Representational means revealed by various physical mechanisms.
  • These in-situ characterization techniques mainly include in-situ electrical performance testing techniques for nanomaterials, in-situ thermal performance testing techniques, and in-situ mechanical property testing techniques.
  • the loads applied in the in-situ mechanical experiments of transmission electron microscopy are usually tensile and compressive loads.
  • the compressive load condition is more suitable for the study of brittle materials (such as ceramics). This is because under the tensile load, the material breaks after the yield point, and the original deformation process cannot be realized. Position observation affects the accurate analysis of the material deformation mechanism.
  • In-situ nanoindentation/compression experiments in TEM have significant advantages over TEM post-station experiments after loading and unloading.
  • the change of the microstructure of the material during indentation could not be observed. It is difficult to derive the correlation between the microstructure and mechanical properties of the material through the microstructure of the segment.
  • the in-situ nanoindentation experiment can observe the change process of the material in the whole process of indenter-stop-withdrawal of the indenter in real time, and can reveal the relationship between the microstructure and mechanical properties of the material from the sub-Aeon, atom and nanometer scale. .
  • the above sample rods have been commercialized by companies such as Hysitron and Nanofactory and have been widely used in in-situ nanoindentation, compression and other experiments to study the mechanical properties of materials under pressure and have achieved outstanding results.
  • the above sample rods are all driven by the piezoelectric effect.
  • the piezoelectric ceramic block is large in volume and can only be placed in the front part of the sample rod, so that the biaxial tilting of the sample cannot be achieved, which makes it difficult to obtain ideal diffraction conditions during the experiment. Thus, it is difficult to observe the microstructure evolution of the material in situ at the atomic and sub-angstrom scales.
  • the invention designs an in situ nanoindentation experimental platform under biaxial tilting condition in a TEM which can be produced in a simple process and can be mass-produced, and can realize nanoindentation, compression and bending of the sample, and in situ through the transmission electron microscope. Recording the evolution of the microstructure during the deformation process provides an advantageous tool for revealing the deformation mechanism of the material.
  • the present invention designs an in situ nanoindentation experimental platform under biaxial tilting conditions in a transmission electron microscope with simple process and mass production.
  • the nanoindentation, compression and bending experiments can be carried out on the sample, and the microstructure evolution during the deformation process is recorded in situ by transmission electron microscopy, which provides a favorable tool for revealing the deformation mechanism of the material.
  • the TEM dual-in-situ in-situ nanoindentation/compression platform is fabricated by semiconductor microfabrication techniques.
  • the driving method used in the compression/indentation experiment may be a hot bimetal, a V-shaped electric beam, a piezoelectric, an electrostatic, an electromagnetic, a memory alloy, or the like. Samples for indentation/compression were prepared by focused ion beam processing and bulk sampling techniques.
  • the integrated platform is bonded to the hot bimetal, and the whole is placed on the stage of the front end of the biaxial tilting heating sample rod. After the energization, the heating crucible on the sample rod heats the driving part.
  • the driving head gradually presses/compresses the sample while achieving in-situ observation of the sub-, atomic and nano-scales of the microstructure evolution of the material under biaxial tilting conditions.
  • the invention solves the limitation that the existing TEM in-situ nanoindentation and compression experiments can not simultaneously achieve biaxial tilting of the sample.
  • the position of the indenter and the sample stage is fixed, and the purpose of controlling the indenter in one dimension can accurately press the sample, thereby reducing the operation difficulty and greatly improving the success rate.
  • observing the evolution process of the microstructure in the material at the sub-Ae, atomic and nanometer scales it is helpful to reveal the deformation mechanism of the material under pressure and establish a corresponding atomic model.
  • a TEM double-dip in-situ nanoindentation platform comprising: a bonding zone, a support beam, a load beam, a sample stage and a micro indenter; wherein the bonding zone is symmetrically distributed on both sides Rectangular plate area; the support beam is 2 ⁇ 4 rectangular fixed beams, connecting the bonding areas on both sides; the load beam is two symmetrical design cantilever beams, one side of each cantilever beam is connected with the bonding area, respectively One side extends toward the center of the device; the sample stage is a flat plate, and the tail end is connected to the end of one of the load beam, close to The micro indenter has a notch as the electron beam transmission region; the micro indenter is a rectangular plate, and the tail end is connected to the other load beam, and has a triangular tip on the side close to the sample stage.
  • the bonding region has a thickness of 5 to 100 ⁇ m and a length and a width of 50 to 200 ⁇ m and 50 to 200 ⁇ m, respectively, for bonding to the driver.
  • the support beam has a thickness of 5 to 100 ⁇ m and a length and a width of 30 to 200 ⁇ m and 5 to 50 ⁇ m, respectively, for connecting the bonding regions on both sides.
  • the load beam has a thickness of 5 to 100 ⁇ m, a length and a width of 10 to 100 ⁇ m and 5 to 100 ⁇ m, respectively, and the free ends respectively carry a micro indenter and a sample stage.
  • micro indenter is connected to the free end of a load beam and has a thickness of 1 to 10 ⁇ m.
  • the sample stage is connected to the free end of the other load beam, and has a thickness of 1 to 10 ⁇ m and a gap of 2 to 20 ⁇ m with the micro indenter for carrying the sample.
  • the platform is integrally formed by semiconductor micro-machining technology, and can be formed at one time, and commonly used materials such as silicon, silicon carbide, diamond, gallium arsenide, quartz crystal and the like are used.
  • the platform can be driven by a hot bimetal, a V-shaped electric beam, a piezoelectric, an electrostatic, an electromagnetic, a memory alloy, or the like.
  • the transmission electron microscope biaxial tilting in-situ nanoindentation/compression experimental platform of the invention comprises five parts: a bonding zone, a support beam, a load beam, a sample stage and a micro indenter.
  • the bonding zone is a region for bonding with the driver on both sides; the supporting beam is connected with the bonding zones on both sides for ensuring the relative position of the indenter and the carrier are unchanged during the bonding process;
  • the load beam is located on the upper edge of the device and is connected to the bonding zone; the indenter and the sample carrier are respectively located at the free ends of the two load beam.
  • the thickness of the bonding zone and the supporting beam should be adjusted according to the mechanical stress experienced during the use of the integrated platform to ensure a firm structure.
  • the load beam thickness is sufficient to hold the sample stage and micro indenter firmly.
  • the microindenter and the sample stage are thinner to reduce the obstruction of the electron beam during biaxial tilting.
  • the thickness of the bonding zone, the support beam and the load beam exceeds 10 ⁇ m, it is necessary to separately reduce the sample stage and the micro indenter to less than 10 ⁇ m.
  • the processing process includes secondary lithography: For the first time, the front mechanical structure is etched, and the overall shape of the device is etched downward; the second time is etched from the back surface to release the window to form an integrated platform.
  • the processing process includes three lithography: the first time is the front micro-indenter and the sample stage area is thinned, and a certain height step is etched from the top to the bottom to ensure the final thickness is less than 10 ⁇ m;
  • the secondary and third lithography processes are the same as when the overall thickness of the platform is less than 10 ⁇ m.
  • the bonding region is a slab region which is symmetrically distributed on the left and right sides of the device, and has a length of 50 to 200 ⁇ m, a width of 50 to 200 ⁇ m, and a thickness of 5 to 100 ⁇ m.
  • the bonding region is a slab region which is symmetrically distributed on the left and right sides of the device, and has a length of 50 to 200 ⁇ m, a width of 50 to 200 ⁇ m, and a thickness of 5 to 100 ⁇ m.
  • two bimetal pieces are firstly fixed in parallel on a copper support ring having an outer diameter of 3 mm, and a metal having a small thermal expansion coefficient is on the inner side, and the two metal pieces are free at the free end when heated. near.
  • the two bonding areas are symmetrically fixed on the hot bimetal sheets on both sides with AB glue, so that the front end of the device is flush with the free end of the bimetal.
  • the supporting beam has 2 to 4 pieces, and is connected to the left and right bonding regions, and has a length of 30 to 200 ⁇ m, a width of 5 to 50 ⁇ m, and a thickness of 5 to 100 ⁇ m. After the bonding is firm, cut all the support beams.
  • the two supporting beams are cantilever beams, the length is 10 to 100 ⁇ m, the width is 5 to 100 ⁇ m, the thickness is 5 to 100 ⁇ m, and the upper edge of the device is located, one end is connected with the bonding area on the same side, and the other end is extended to the middle of the device. , for the free end, used to carry the micro indenter and the sample carrier.
  • the micro indenter is connected to the free end of a load beam and has a thickness of 1 to 10 ⁇ m.
  • the sample stage is connected to the free end of the other load beam and has a thickness of 1 to 10 ⁇ m.
  • the distance between the micro indenter and the sample stage is 2 to 20 ⁇ m.
  • the sample is soldered to the sample stage using focused ion beam techniques.
  • the temperature of the bimetal driver is controlled by changing the heating current of the heating rod; the bimetal is bent at the free end due to the difference in thermal expansion coefficients of the two metals during the heating process, and is close to each other, driving the indentation/compression head and the sample stage Close to each other until the indenter is pressed into the thin area.
  • the indenter depth and speed can be adjusted by controlling the rate of temperature increase.
  • the microstructure of the thin region during the pressing process was observed and recorded in real time through a transmission electron microscope observation screen or a CCD camera.
  • In situ mechanical experiments such as in-situ compression and in-situ bending can be achieved by changing the size and shape of the indenter and sample.
  • the front end of the indenter used for the indentation test is designed to be pointed, and the corresponding sample shape is designed as a sheet; the head for compression or bending is designed to be flat, and can be square or rectangular.
  • the corresponding sample is designed as a column with a cross-sectional area smaller than the cross-sectional area of the flat head.
  • the in-situ tensile test of the sample can be performed on the platform by changing the bonding direction of the driving bimetal so that the two free ends are away from each other during heating.
  • the present invention provides a platform for in-situ nanoindentation experiments under the condition of double tilting of a transmission electron microscope, and fills in the blank of the indirect indentation test in the transmission electron microscope.
  • the TEM in-situ nanoindentation platform involved in the present invention can be driven in a variety of ways.
  • the drive and control method is simple when selecting a hot bimetal drive.
  • the in-situ nanoindentation system can be directly used with commercial TEM heating rods for easy operation.
  • the TEM in-situ nanoindentation platform involved in the present invention provides a suitable positional relationship between the indenter and the sample, and only needs to control the driving system to drive the indenter and the sample in one dimension to achieve indentation, compression, and The bending experiment improves the working efficiency and the success rate of the experiment.
  • the in-situ nanoindentation platform involved in the present invention can preset the experimental temperature range when the sample is loaded with the focused ion beam, and can meet the requirements of the force-heat coupling experiment to some extent.
  • Figure 1 is a schematic diagram of a TEM double-in-situ nanoindentation platform.
  • Figure 2 is an assembled view of a TEM double-indentation in-situ nanoindentation platform and a bimetal driver.
  • FIG. 3 Photograph of in situ nanoindentation experiment (a) before indentation; (b) indentation process; (c) after indentation.
  • FIGS. 1 and 2 The present invention will be further described below in conjunction with FIGS. 1 and 2:
  • the first lithography uses dry etching, first from the front side of the sample stage and micro indenter area The etch is a certain depth, so that the final thickness of the region is less than 10 ⁇ m; the second lithography uses dry etching to etch the integrated structure from the front side; the third lithography uses wet etching, from the back side Release the window and etch until the entire device is left floating.
  • the overall thickness of the platform is less than 10 ⁇ m, only the last two steps of photolithography are performed.
  • the specific method is as follows: taking the bimetal drive as an example, the functional area of the device is facing up and sticking to the front end of the bimetal driver inward of the passive end; after the bonding is firm, the support beam is cut off, so that both sides of the indenter and the sample carrier are completely Separation; the sample is removed, adhered to the stage, and thinned using a focused ion beam bulk sampling technique.
  • the above-mentioned TEM in-situ nanoindentation platform equipped with a sample is placed in a double-tilt heated sample rod of a transmission electron microscope, inserted into a transmission electron microscope, and the sample is tilted to a desired angle, and can be selected in a bright field or a dark field.
  • the driving part is heated in the field or in the diffraction mode, and the deformation process of the recorded sample under the action of the indenter is observed in real time.

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Abstract

一种透射电镜双倾原位纳米压痕平台属于纳米材料力学性能-显微结构原位表征领域。该平台主要由粘接区(1)、支撑梁(2)、承载梁(3)、样品载台(5)与微型压头(4)组成，整体结构通过半导体微细加工技术制备。原位纳米压痕实验可采用热双金属片(7)、V型电热梁、压电、静电、电磁、记忆合金等方式进行驱动，样品通过聚焦离子束块体取样技术获得。该一体化平台可置于透射电镜(TEM)样品杆前端的狭小空间内，在双轴倾转条件下，驱动装置驱动微型压头(4)，在透射电镜中对材料进行原位纳米压痕、原位压缩和原位弯曲等实验。可以在亚埃、原子和纳米尺度下对材料的变形过程进行原位观察，研究其变形机制，揭示其显微结构与力学性能的关系。

Description

一种透射电镜双倾原位纳米压痕平台 技术领域
本发明涉及一种在透射电镜中，在双轴倾转条件下对材料进行原位纳米压痕、压缩、弯曲等实验的平台。通过透射电镜实现对样品变形过程中显微结构演变的亚埃、纳米、原子尺度观测。属于透射电镜中纳米材料力学性能-显微结构原位表征领域。
背景技术
当材料特征尺寸降至纳米、原子级别时，利用传统的理论无法解释纳米材料的各种性能。纳米材料的力学性能、显微结构及其之间的相关性具有区别于块体材料的独特性。例如，Kiritan等在《Anomalous production of vacancy clusters and the possibility of plastic deformation of crystalline metals without dislocations》中发现面心结构块体材料的变形机制主要为位错滑移，而在纳米尺度的面心结构薄膜中，变形与材料内部大量的空位密切相关；Zheng等在《discrete plasticity in sub-10-nm-sized gold crystals》中发现10nm以下的单晶金中，主导塑形变形的机制为不全位错形核，区别于金的体材料中由Frank-Read源主导的塑形变形机制；Yu等在《strong crystal size effect on deformation twinning》中发现微米尺寸TiAl合金柱在压缩时的塑性变形以孪生变形为主，与宏观材料相同。而当尺寸减小到亚微米量级时，变形则以位错滑移为主。可见，研究材料微观变形机制及其对力学性能的影响对于提高纳米材料制备和应用水平具有很大的理论和实际意义。
透射电子显微镜(TEM)可以在亚埃、纳米、原子尺度研究材料的微观结构，最新的球差透射电子显微镜已可以实现在空间分辨率小于0.1nm的条件下研究材料的显微结构。除基本的显微结构表征外，国际上研究者和仪器厂家亦 发展了各种结合TEM的原位表征技术，用于研究材料的显微结构和各种性能的相关性，包括材料的力学、热学、电学、光学以及多种耦合性能，极大丰富了对材料各种物理机制揭示的表征手段。这些原位表征技术主要有纳米材料的原位电学性能测试技术、原位热学性能测试技术和原位力学性能测试技术。其中纳米材料的原位力学测试方法和设备的发展受到了广泛的关注。这是由于材料的力学性能决定了材料服役的稳定性和使用寿命，研究材料在外力条件下的显微结构演变对于理解材料的弹/塑性变形机理，发展高性能材料具有十分重要的指导意义。
目前透射电镜原位力学实验中施加的载荷通常为拉伸和压缩载荷。相比于拉伸载荷，压缩载荷条件更适用于脆性材料(如陶瓷)的研究，这是由于在拉伸载荷下，材料在屈服点后即发生断裂，不能实现对其塑形变形过程的原位观察，影响对材料变形机制的精确分析。
在TEM中进行原位纳米压痕/压缩实验与载荷卸载后再进行观察分析的TEM后位实验相比具有明显的优势。后位实验中无法观察到压头压入时材料微观结构的变化过程，难以通过片段的显微结构推导材料显微结构-力学性能的相关性。原位纳米压痕实验可以实时观察分析材料在压头压入-停留-撤出的整个过程中的变化过程，可以直观地从亚埃、原子、纳米尺度揭示材料显微结构-力学性能的关系。
目前研究中的原位纳米压缩/压痕实验主要是通过商业化的原位纳米压缩/压痕样品杆进行。1998年Wall和Dahmen在《an in-situ nanoindentation specimen holder for a high-voltage transmission electron microscope》一文中设计了第一代适用于高压透射电镜的原位纳米压痕样品杆，采用可拆卸的样品搭载台和压电驱动压头，通过齿轮电机粗调机构将压头调整到距样品一定范围内，再用压电陶瓷驱动使压头进一步靠近并压入样品。2001年Stach和Freeman等在《development of a nanoindenter for in situ transmission electron microscopy》一文中将这一样品杆应用于低压电镜，同时改进了压头的位移分辨率，使压入过程更加稳定可控。作者使用这种样品杆对金属和非金属薄膜材料进行了 压痕实验。2003年Svensson和Jompol等在《compactdesign of a transmission electron microscope-scanning tunneling microscope holder with three-dimensional coarse motion》一文中通过使用压电陶瓷位移积累方式进行粗调，消除了早期样品杆由于粗调电机工作引入的振动。2006年Bobji和Ramanujan等在《a miniaturized TEM nanoindenter for studying material deformation in situ》一文中进一步提高了对压入轨迹的控制，同时加入了可控的柔性铰链力信号传感器，可以获得压入过程的力-位移曲线。上述原位纳米压痕实验中压头形状为曲率半径几十到几百纳米的锥形，样品薄区为几十到几百纳米厚的电子束透明区，在透射电镜中无法观察到二者的“高度”关系。上述原位纳米压痕实验中通过外部驱动电机或压电陶瓷靠近样品非常耗时。2010年Lockwood和Wedekind等在《advanced transmission electron microscope triboprobe with automated closed-loop nanopositioning》一文中发展了一种图像反馈系统，可以自动完成透射原位实验中的纳米级精确定位，解决了压头样品难以对正的问题。
上述样品杆已经由Hysitron和Nanofactory等公司推出商业化的产品并大量应用于原位纳米压痕、压缩等实验中，研究材料在压力状态下的力学性能并取得了突出的成果。上述样品杆均利用压电效应进行驱动，压电陶瓷块体积较大，只能放置在样品杆中前部，因而无法实现样品的双轴倾转，导致实验过程中很难获得理想的衍射条件，从而难以实现在原子和亚埃尺度下原位观察材料的显微结构演化。北京工业大学的韩晓东等在专利《透射电镜用原位双轴倾转纳米压痕仪》(专利申请号：201320574347.8)中设计了一种可以在透射电镜中实现双轴倾转条件下的原位纳米压痕的平台，设计简单，成本低廉；但难以将压头精确定位到样品上合适位置。
本发明设计了一种工艺简单、可批量化生产的透射电镜中双轴倾转条件下原位纳米压痕实验平台，可以实现对样品进行纳米压痕、压缩和弯曲，同时通过透射电镜原位记录变形过程中的显微结构演变，为揭示材料的变形机理提供有利工具。
发明内容
针对现有透射电镜原位纳米压痕/压缩平台中存在的各种问题，本发明设计了一种工艺简单、可批量化生产的透射电镜中双轴倾转条件下原位纳米压痕实验平台，可以实现对样品进行纳米压痕、压缩和弯曲实验，同时通过透射电镜原位记录变形过程中的显微结构演变，为揭示材料的变形机理提供有利工具。
该透射电镜双倾原位纳米压痕/压缩平台通过半导体微细加工技术制得。压缩/压痕实验所用驱动方式可采用热双金属片、V型电热梁、压电、静电、电磁、记忆合金等。用于压痕/压缩的样品通过聚焦离子束加工及块体取样技术制得。
以热双金属片驱动为例，将一体化平台粘接在热双金属片上，整体置于双轴倾转加热样品杆前端的载台上，通电后样品杆上的加热坩埚对驱动部分加热，驱动压头逐渐压入/压缩样品，同时在双轴倾转条件下，实现对材料显微结构演化的亚埃、原子和纳米尺度的原位观察。
本发明解决了现有透射电镜原位纳米压痕、压缩实验无法同时实现样品双轴倾转的缺限。同时压头与样品载台位置固定，实现在一维方向上控制压头即可准确压入样品的目的，减小了操作困难，极大提高了成功率。同时在亚埃、原子和纳米尺度下观察材料内显微结构的演化过程，有助于揭示压力作用下材料的变形机制和建立对应的原子模型。
本发明中实现上述目的的途径如下所述：
一种透射电镜双倾原位纳米压痕平台，其特征在于：包括粘接区、支撑梁、承载梁、样品载台和微型压头五部分；其中，粘接区为位于两侧呈对称分布的矩形平板区；支撑梁为2～4根矩形固支梁，连接两侧的粘接区；承载梁为两根对称设计的悬臂梁，每根悬臂梁一侧分别与粘接区相连，另一侧伸向器件中心；样品载台为一块平板，尾端与其中一根承载梁的末端相连，靠近 微型压头一侧切有缺口作为电子束透过区；微型压头为一块矩形平板，尾端与另一根承载梁相连，在靠近样品载台一侧有一个三角形尖头。
进一步，所述的粘接区厚度为5～100μm，长和宽分别为50～200μm和50～200μm，用于与驱动器粘接。
进一步，所述的支撑梁厚度为5～100μm，长度和宽度分别为30～200μm和5～50μm，用于连接两侧粘接区。
进一步，所述的承载梁厚度为5～100μm，长度和宽度分别为10～100μm和5～100μm，自由端分别承载微型压头和样品载台。
进一步，所述的微型压头与一根承载梁的自由端相连，厚度为1～10μm。
进一步，所述的样品载台与另一根承载梁的自由端相连，厚度为1～10μm，与微型压头间隙为2～20μm，用于搭载样品。
进一步，所述平台采用半导体微细加工技术一体化成形制备，可一次成形，选用硅、碳化硅、金刚石、砷化镓、石英晶体等微电子机械系统常用材料。
进一步，平台可选用热双金属片、V型电热梁、压电、静电、电磁、记忆合金等方式进行驱动。
本发明所述的透射电镜双轴倾转原位纳米压痕/压缩实验平台包括粘接区、支撑梁、承载梁、样品载台和微型压头五部分。所述的粘接区为两侧用于与驱动器粘接的区域；所述的支撑梁与两侧粘接区连接，用于在粘接过程中保证压头和载台的相对位置不变；所述的承载梁位于器件上沿，与粘接区相连；所述的压头和样品载台分别位于两根承载梁的自由端。粘接区和支撑梁的厚度需根据一体化平台使用过程中所承受的机械应力进行调整，保证结构坚固。承载梁厚度需足以稳固地承载样品载台和微型压头。微型压头和样品载台的厚度较薄，以减小双轴倾转时对电子束的遮挡。当粘接区、支撑梁和承载梁厚度超过10μm时，需要对样品载台和微型压头单独进行减薄，减至10μm以下。
具体地说，当平台整体厚度小于10μm时，其加工工艺包括二次光刻： 第一次为正面机械结构刻蚀，向下刻蚀出器件整体外形；第二次从背面刻蚀，释放窗口，形成一体化平台。当平台整体厚度超过10μm时，加工工艺包括三次光刻：第一次为正面微型压头和样品载台区域减薄，从上向下刻蚀出一定高度的台阶，保证最终厚度小于10μm；第二次与第三次光刻过程与平台整体厚度小于10μm时相同。
所述的粘接区为分布于器件左右两侧对称的平板区，长度为50～200μm，宽度为50～200μm，厚度为5～100μm。以热双金属驱动方式为例，使用时，先将两个双金属片平行固定于外径为3mm的铜支撑环上，热膨胀系数较小的金属处于内侧，加热时两根金属片自由端相互靠近。用AB胶将两个粘接区对称地固定在两侧的热双金属片上，使器件前端与双金属片自由端平齐。所述的支撑梁有2～4根，连接左右粘接区，长度为30～200μm，宽度为5～50μm，厚度为5～100μm。粘接牢固后，将所有支撑梁切断。所述的两根承载梁为悬臂梁，长度为10～100μm，宽度为5～100μm，厚度为5～100μm，位于器件上沿，一端与同侧的粘接区相连，另一端伸向器件中间，为自由端，分别用于承载微型压头和样品载台。所述的微型压头与一根承载梁的自由端相连，厚度为1～10μm。所述的样品载台与另一根承载梁的自由端相连，厚度为1～10μm。微型压头与样品载台间距2～20μm。用聚焦离子束技术将样品焊接于样品载台上。
通过改变加热杆的加热电流，控制双金属片驱动器的温度；双金属片在升温过程中由于两种金属热膨胀系数不同导致自由端发生弯曲，相互靠近，驱动压痕/压缩压头和样品载台相互靠近，直至压头压入薄区。通过控制升温速率可以调节压头压入深度和速度。通过透射电镜观察屏或CCD相机实时观察、记录薄区在压入过程中显微结构的变化。
通过改变压头和样品的尺寸和形状，可实现原位压缩和原位弯曲等其它透射电镜原位力学实验。用于压痕实验的压头前端设计为劈尖状，对应的样品形状设计为薄片状；用于压缩或弯曲的压头设计为平头状，可为正方或长方形。对应的样品设计为柱状，其截面积小于平头压头的截面积。
改变驱动双金属片的粘接方向，使加热时两自由端相互远离，即可在此平台上进行样品的原位拉伸实验。
本发明有如下优点：
1.本发明提供了一种可以实现透射电镜双倾条件下的原位纳米压痕实验的平台，填补了透射电镜中无法实现双倾原位压痕实验的空白。
2.本发明中涉及的透射电镜原位纳米压痕平台可通过多种方式进行驱动。选择热双金属驱动时，驱动和控制方法简单。搭建的原位纳米压痕系统可以直接与商业化透射电镜加热杆配合使用，操作便捷。
3.本发明中涉及的透射电镜原位纳米压痕平台本身提供了压头和样品合适的位置关系，仅需控制驱动系统在一维方向上驱动压头和样品即可实现压痕、压缩、弯曲实验，提高了工作效率和实验的成功率。
4.本发明中涉及的原位纳米压痕平台可以在用聚焦离子束搭载样品时预设实验温度范围，可以一定程度上满足力热耦合实验的要求。
附图说明
图1透射电镜双倾原位纳米压痕平台示意图。
图中图面说明如下
1粘接区  2支撑梁  3承载梁  4微型压头  5样品载台
图2透射电镜双倾原位纳米压痕平台与双金属片驱动器组装图。
图中图面说明如下
6铜支撑环  7双金属片
图3原位纳米压痕实验照片(a)压头压入前；(b)压头压入过程中；(c)压头退出后。
具体实施方式：
下面结合图1、图2对本发明做进一步说明：
制备具体方法：利用半导体微细加工技术，当平台整体厚度超过10μm时，分三次光刻：第一次光刻使用干法刻蚀，先从正面将样品载台和微型压头所在区域向下刻蚀一定深度，使该区域最终厚度小于10μm；第二次光刻使用干法刻蚀，从正面向下刻蚀出一体化平台整体结构；第三次光刻使用湿法刻蚀，从背面向上释放窗口，刻蚀至整个器件悬空。当平台整体厚度小于10μm时，只需进行后两步光刻。
使用具体方法：以双金属片驱动为例，将器件功能区朝上，粘在被动端向内的双金属片驱动器前端；粘接牢固后切断支撑梁，使压头和样品载台两侧完全分离；用聚焦离子束块体取样技术将样品取出、粘在载台并减薄。
实验具体方法：将上述搭载有样品的的透射电镜原位纳米压痕平台装入透射电镜双倾加热样品杆中，插入透射电镜，将样品倾转至理想的角度，可选择在明场、暗场或者衍射模式下对驱动部分进行加热，实时观察记录样品在压头作用下的变形过程。

Claims (8)

  1. 一种透射电镜双倾原位纳米压痕平台，其特征在于：包括粘接区、支撑梁、承载梁、样品载台和微型压头五部分；其中，粘接区为位于两侧呈对称分布的矩形平板区；支撑梁为2～4根矩形固支梁，连接两侧的粘接区；承载梁为两根对称设计的悬臂梁，每根悬臂梁一侧分别与粘接区相连，另一侧伸向器件中心；样品载台为一块平板，尾端与其中一根承载梁的末端相连，靠近微型压头一侧切有缺口作为电子束透过区；微型压头为一块矩形平板，尾端与另一根承载梁相连，在靠近样品载台一侧有一个三角形尖头。
  2. 根据权利要求1所述的一种透射电镜双倾原位纳米压痕平台，其特征在于：所述的粘接区厚度为5～100μm，长和宽分别为50～200μm和50～200μm，用于与驱动器粘接。
  3. 根据权利要求1所述的一种透射电镜双倾原位纳米压痕平台，其特征在于：所述的支撑梁厚度为5～100μm，长度和宽度分别为30～200μm和5～50μm。
  4. 根据权利要求1所述的一种透射电镜双倾原位纳米压痕平台，其特征在于：所述的承载梁厚度为5～100μm，长度和宽度分别为10～100μm和5～100μm。
  5. 根据权利要求1所述的一种透射电镜双倾原位纳米压痕平台，其特征在于：所述的微型压头厚度为1～10μm。
  6. 根据权利要求1所述的一种透射电镜双轴倾原位纳米压痕平台，其特征在于：所述的样品载台与另一根承载梁的自由端相连，厚度为1～10μm，与微型压头间隙为2～20μm。
  7. 根据权利要求1所述的一种透射电镜双倾原位纳米压痕平台，其特征在于：平台采用半导体微细加工技术一体制备成形，选用硅、碳化硅、金刚石、砷化镓或石英晶体。
  8. 根据权利要求1所述的一种透射电镜双轴倾原位纳米压痕平台，其特征在于：平台选用热双金属片、V型电热梁、压电、静电、电磁或记忆合金方式进行驱动。
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